CN115003171A - 食品添加剂和其制备方法 - Google Patents
食品添加剂和其制备方法 Download PDFInfo
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- CN115003171A CN115003171A CN202080074456.6A CN202080074456A CN115003171A CN 115003171 A CN115003171 A CN 115003171A CN 202080074456 A CN202080074456 A CN 202080074456A CN 115003171 A CN115003171 A CN 115003171A
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Abstract
本公开涉及一种用于改善类胡萝卜素组合物的感官特性的方法,所述方法包含:将类胡萝卜素组合物提供到反应容器中;以及将所述类胡萝卜素组合物保持在50℃到180℃之间的保持温度下,同时从所述反应容器中清除气氛,持续适于从所述类胡萝卜素组合物中去除引起气味的挥发性杂质的时间。本公开还涉及根据以上方法制备的类胡萝卜素食品添加剂调配物。
Description
技术领域
本公开涉及用于制备食品添加剂组合物的方法以及含有所述食品添加剂组合物的食品和饮料。具体而言,本公开涉及具有改善的感官品质的适于食品和饮料使用的β-胡萝卜素和其它类胡萝卜素产品。
背景技术
合成偶氮染料黄色5号(yellow 5)和黄色6号(yellow 6)是通常使用的食品着色剂。然而,由于消费者偏好,商业食品行业趋向于远离合成颜色和风味添加剂并转向被视为“天然”的食品产品。因此,越来越多地使用植物来源的化合物作为颜色和风味添加剂。
类胡萝卜素是适于此类目的的600多种碳氢化合物(胡萝卜素)中的一种类别。例如,通过引用以其整体并入的US 9,375,387描述了适于动物和人类食品、膳食补充剂、化妆品组合物和药物使用的类胡萝卜素组合物。
类胡萝卜素是负责许多植物、水果和花卉的颜色的色素。类胡萝卜素是典型的具有双键和其他化学基团的C30-C40化合物,这些化学基团可以使其为反应性的并易于分解为较小分子量的化合物,从而产生各种香气。例如,C9到C13化合物,如β-紫罗酮(C13)等,是与花和植物气味有关的化合物(参见John C.Leffingwell博士的“作为香味和香气前体的类胡萝卜素:综述(Carotenoids as Flavor&Fragrance Precursors:A Review)”。类胡萝卜素作为维生素A的来源在人类营养中也很重要并且被认为有助于预防癌症和心脏病。因此,期望由类胡萝卜素开发天然食品添加剂以获得令人愉悦的感官属性,包括颜色和最小的气味。
发明内容
本公开的各方面涉及一种用于改善类胡萝卜素食品添加剂调配物的感官特性的方法,所述方法包括:将类胡萝卜素组合物提供到反应容器中;以及将所述类胡萝卜素组合物保持在50℃到180℃之间的保持温度下,同时从所述反应容器中清除气氛持续合适的时间,以从所述类胡萝卜素组合物中去除引起气味的挥发性杂质。
本公开的各方面还涉及具有改善的感官性质的类胡萝卜素食品添加剂调配物。
具体实施方式
β-胡萝卜素和其它类胡萝卜素用作食品添加剂,尤其用于对食品和饮料增强营养、调味和着色。商业β-胡萝卜素以及含有α-胡萝卜素、番茄红素、叶黄素和β-阿朴胡萝卜醛的类胡萝卜素产品表现出不同的气味。除了具有独特气味外,现有商业产品可能会使食品和饮料的颜色呈现为橙色。虽然商业类胡萝卜素食品添加剂的气味和颜色对于许多当前应用来说是可接受的或甚至是理想的,但还有一些应用期望更小的气味和/或更黄的颜色。
本公开提供用于产生与现有类胡萝卜素产品相比表现出改善的感官性质的类胡萝卜素食品添加剂调配物的方法。改善的感官性质使类胡萝卜素用于可能不期望气味和/或橙色颜色的更多种食品、饮料和膳食补充剂产品中。
虽然不希望受理论的束缚,但据信,市售类胡萝卜素食品添加剂中的至少一部分的“变味”是由于杂质的存在,尤其是小分子量挥发性降解化合物的存在,所述杂质可能是类胡萝卜素化合物的合成过程或降解的副产物。因此,虽然许多类胡萝卜素化合物与其自身的气味相关,但类胡萝卜素组合物中存在降解产物可能导致过多或不期望的气味或颜色。当商业合成或天然来源的类胡萝卜素食品添加剂中存在此类化合物时,足以去除挥发性降解化合物和其它杂质的处理被认为会减少类胡萝卜素食品添加剂中引起气味的组分的总量并使感官性质得到改善。基于此理论,本公开涉及用于使用类胡萝卜素组合物制备食品添加剂调配物的方法,所述类胡萝卜素组合物减少挥发性降解化合物和其它杂质的量,以在更小的气味、比橙色更黄的颜色方面提供改善的感官性质。
适于用作起始材料的类胡萝卜素组合物包括包含以下中的至少一种的类胡萝卜素组合物:β-胡萝卜素、番茄红素、胭脂素(bixin)、玉米黄素、隐黄素、柠檬黄素、叶黄素、角黄素、虾青素、β-阿朴-4'-胡萝卜醛、β-阿朴-8'-胡萝卜醛、β-阿朴-12'-胡萝卜醛、β-阿朴-8'-胡萝卜素酸(carotenic acid)以及此组中含羟基代表物和含羧基代表物的酯,例如低级烷基酯,并且优选地为甲酯和乙酯。特别优选地,使用工业上容易获得的代表物,例如β-胡萝卜素、角黄素、虾青素、番茄红素、β-阿朴-8'-胡萝卜醛和β-阿朴-8'-胡萝卜素酸酯,它们可以单独地或以混合物的形式使用。类胡萝卜素可以是天然来源的或商业合成的“天然等同物”,这意味着活性成分在化学上与天然存在的类胡萝卜素相同。β-胡萝卜素是优选的。合适的β-胡萝卜素可以(巴斯夫集团(BASF SE)的商标)商购获得。
如以上所提到的,据信商业类胡萝卜素组合物含有一种或多种引起变味的杂质,如微量挥发性小分子和降解产物等。因此,本文提及“类胡萝卜素组合物”涵盖包括小部分杂质的组合物并且不应被解释为是指所期望的类胡萝卜素的天然存在的分子本身或仅由所期望的类胡萝卜素分子组成的纯组合物。
类胡萝卜素组合物可以呈粉末、溶液、悬浮液、乳液、分散体和小珠的形式或其它市售形式。在不背离本公开的情况下,类胡萝卜素组合物可以含有用于制备市售类胡萝卜素组合物的一种或多种溶剂、稀释剂、赋形剂、载体、分散剂等。实例包括淀粉、植物来源的胶、明胶、油、糖、树脂、脂肪、蜡、软化剂和无机填料等。
在一些实施方案中,类胡萝卜素组合物可以呈适于动物和/或人类营养的在任何食用油中的含油性分散体的形式。所述食用油可以是合成油、矿物油、植物油或动物来源的油。合适的植物油的实例包括但不限于大豆油、棕榈油、棕榈仁油、葵花油、玉米油、亚麻籽油、棉籽油、生育酚、菜籽油、红花油、小麦胚芽油、米糠油、椰子油、扁桃油、杏仁油、鳄梨油、荷荷巴油、榛子油、核桃油、花生油、开心果油和植物来源的中链脂肪酸甘油三酯(MCT油)。合适的合成油包括但不限于半合成甘油三酯,如Miglyol型等的辛酸/癸酸甘油三酯,以及动物脂硬脂酸甘油酯、液体石蜡、硬脂酸甘油酯、肉豆蔻酸异丙酯、己二酸酯、二异丙基酯、2-己酸乙酯、硬脂酰乙酰酯、液态氢化聚异丁烯、角鲨烷、角鲨烯。合适的动物油包括油和脂肪,如猪油、牛油、鱼油(包括鲭鱼油、鲱鱼油、金枪鱼油、大比目鱼油、鳕鱼油和鲑鱼油),鱼油和诸如南美鲱鱼油、北欧鲱鱼油等的鱼油的市售混合物,以及绵羊油。一种或多种油的混合物也是合适的。特别优选植物油,如大豆油、棕榈油、棕榈仁油、葵花油、红花油、玉米油、橄榄油、亚麻子油、菜籽油、米糠油、椰子油、花生油、MCT油和其混合物。
在油溶液和/或悬浮液的实施方案中,油的总量未进行限制,并且可以占油溶液和/或悬浮液的至多99重量%,或优选地至多60重量%,或更优选地至多50重量%。
为了保护类胡萝卜素组合物中的类胡萝卜素免受氧化分解,可以另外包含稳定剂和抗氧化剂。常用抗氧化剂的实例包括但不限于维生素E、维生素C、丁基化羟基甲苯、丁基化羟基茴香醚、抗坏血酸棕榈酸酯、抗坏血酸、抗坏血酸钠以及d,1-α-生育酚和d,1-α-生育酚酯。
下面讨论用于制备具有改善的感官性质的合适的类胡萝卜素食品添加剂的方法。所述方法旨在去除或减少挥发性杂质和降解产物的量。
用于改善类胡萝卜素组合物的感官性质的优选方法包括使类胡萝卜素组合物连同任何分散剂、添加剂等经受保持,同时用惰性气体清除和/或喷射以从类胡萝卜素组合物中除去已挥发的挥发性化合物。所述方法可以在任何合适的反应容器中执行。
所述保持步骤包括将类胡萝卜素组合物保持适于去除足够量的已挥发的引起气味的挥发性杂质的时间,以改善类胡萝卜素组合物相对于未经处理的类胡萝卜素组合物的感官性质。优选地,该保持步骤在50℃与180℃之间、更优选地在70℃与110℃之间、甚至更优选地在80℃与100℃之间或其间的任何温度的保持温度下发生。
适于去除足够量的已挥发的引起气味的挥发性杂质的保持时间的长度取决于保持温度,因为温度可能影响小分子挥发的速率。较高温度能够需要较短的保持时间,而较低温度则可能需要较长的保持时间。在一些实施方案中,保持时间可以为至少30分钟或更长,优选至少2小时或更长,或者甚至更优选至少3小时或更长。保持时间的上限一般未进行限制,并且可以被设定为4小时或高达12小时或更长。
所述保持步骤至少部分地与气氛清除结合以从反应容器中除去引起气味的挥发性杂质。优选地,所述保持步骤与从反应容器中持续清除气氛同时进行。
反应容器的气氛可以通过适于从反应容器中除去已挥发的挥发性化合物的任何方法进行清除,包括但不限于在从反应容器中排出气氛的同时将惰性气体引入到反应容器中。惰性气体的非限制性实例包括氮气、二氧化碳和蒸汽或其组合。优选地,清除包括氮气喷射,用于将氮气引入到反应容器中的类胡萝卜素组合物中。另外或可替代地,所述反应容器可以经受真空或减压(低于1atm)以从类胡萝卜素组合物中除去已挥发的挥发性化合物。
任选地,所述方法可以进一步包括在保持之前或之后执行的热处理步骤。在该热处理步骤中,优选地将类胡萝卜素组合物加热到足以溶解或熔化类胡萝卜素组合物的最低温度。优选地,热处理温度的上限低于类胡萝卜素降解的温度。合适的热处理温度可以介于130℃与250℃之间、更优选地介于150℃与225℃之间、甚至更优选地介于170℃与180℃之间或其间的任何温度。热处理的持续时间未进行限制,但适当地可以为40分钟或更短,更优选30分钟或更短,更优选20分钟或更短,或更优选10分钟或更短。
优选地,所述热处理还至少部分地与从反应容器中清除气氛一起执行。甚至更优选地,热处理步骤与从反应容器中持续清除气氛同时执行。
适于改善类胡萝卜素组合物的感官性质的方法可以进一步包括执行结晶步骤以充分减少结晶产物中存在的挥发性降解产物的量。另外,对类胡萝卜素组合物进行处理可以包括在有或没有减压,有或没有如氮气、蒸汽或溶剂等汽提剂的情况下升高温度一段时间,以减少挥发性降解产物的含量。另外或可替代地,可以使用如刮膜蒸发、降膜蒸发的蒸发技术,其中添加或未添加如氮气、蒸汽或溶剂的汽提剂,以去除足够量的挥发性降解产物,并由此改善类胡萝卜素组合物的感官性质。另外或可替代地,类胡萝卜素组合物可以经受蒸馏以除去足够量的挥发性降解产物。
去除“足够量”的已挥发的引起气味的挥发性杂质以改善类胡萝卜素组合物的感官性质可以通过评价已处理的类胡萝卜素组合物的气味和颜色来评估。
去除足够量的已挥发的引起气味的挥发性杂质以改善类胡萝卜素组合物的感官性质的评估可以根据本领域已知的方法使用感官小组来执行。合适的感官评价是《感官评 价技术(Sensory Evaluation Techniques)》第2版Meilgaard,Civile,Carr 1991第81-88页中描述的差异测试,该文献通过引用并入本文。在差异测试中,感官小组将具有1ppm到6ppm类胡萝卜素的类胡萝卜素组合物的气味与无气味对照(即黄色5号)进行比较,以评价类胡萝卜素组合物的气味强度。小组成员还针对自身对对照进行评价以评估结果的准确性。
气味的强度按0到10的等级排序,其中0为与对照相比没有差异,而10表示极端差异。收集由十个人(N=10)指定的排序值并求平均以得出气味强度值。
去除“足够量”的已挥发的引起气味的挥发性杂质以改善类胡萝卜素组合物的感官性质通常对应于不大于5、优选地不大于4的气味强度值。
另外或可替代地,去除足够量的已挥发的杂质以改善类胡萝卜素组合物的感官性质的评估也可以使用气相色谱(GC)顶空分析来执行。
优选地,处理后的类胡萝卜素组合物的颜色可以类似于黄色5号(即酒石黄),其为黄色色素。因此,在处理之后,类胡萝卜素组合物可以吸收可见区域中的类似于黄色5号的光。
类胡萝卜素食品添加剂调配物可以通过本领域已知的技术调配为油悬浮液或溶液、粉末、乳液、分散体、小珠等。类胡萝卜素食品添加剂的形式可能会影响组合物中类胡萝卜素的合适量。例如,合适的油溶液可以含有量为至多30重量%、至多20重量%或至多15重量%的一种或多种类胡萝卜素。一种或多种类胡萝卜素的量取决于所需应用并且可以由本领域的技术人员选择。
实施例
实施例1:制备12%β-胡萝卜素油悬浮液
表1
目标 | 实验 | 活性% | |||||
项目# | 材料 | 批号 | 重量% | g | 重量 | 重量 | 最终 |
活性 | |||||||
1 | MCT | 53.80% | 96.84 | 96.84 | 102.20 | ||
2 | Lucarotin 30% | 40.00% | 72.00 | 22.320 | 76.160 | 12.40% | |
3 | α-生育酚 | 6.20% | 11.16 | 10.83 | 12.30 | 6.01% | |
总计1-3 | 100.00% | 180.00 | |||||
总计1-3(实际) | 190.66 | ||||||
目标批次大小g | 180.00 |
用氮气喷射清除反应器,并在排气扇下保持清除,同时使混合物经受热处理并保持在表2中列出的条件下。
表2
时间(小时:分钟) | 温度(℃) |
0:00 | 25 |
0:05 | (NR) |
0:10 | 89 |
0:15 | 136 |
0:18 | 142 |
0:21 | 158 |
0:24 | 156 |
0:25 | 159 |
0:26 | 162 |
0:27 | 163 |
0:28 | 164 |
0:30 | 164 |
0:32 | 162 |
0:34 | 158 |
0:39 | 148 |
1:04 | 101 |
1:30 | 73 |
2:00 | 94 |
2:16 | 82 |
2:37 | 94 |
2:40 | 97 |
2:50 | 90 |
3:11 | 72 |
3:22 | 66 |
3:55 | 87 |
4:13 | 87 |
此后,使反应器的内容物冷却,然后在温度下降到50℃以下时进行倾析。
实施例2:制备乳液
使用实施例1中制备的12%β-胡萝卜素油悬浮液(12%BC油)以使用表3中示出的材料和组分的量制备0.975%β-胡萝卜素乳液。
表3
乳液 | 量(g) |
OSI淀粉(胶囊) | 152.2 |
抗坏血酸 | 0.43 |
柠檬酸 | 1.42 |
12%BC油 | 31.5 |
山梨酸钾 | 0.45 |
水 | 216.5 |
总计 | 400.63 |
将山梨酸酯淀粉在50℃的水中混合5分钟,然后添加抗坏血酸和柠檬酸,然后混合,持续总计60分钟,直至形成澄清溶液。将12%BC油(约50℃)倾倒在淀粉溶液的顶部,并且在加热到60℃的条件下用旋转螺杆混合器将混合物混合2分钟。然后使混合物在50bar下经受高压均质化。将所得乳液储存在室温下。
对乳液的观察表明在高压均质化之前可能在乳液的顶部存在非常少量的黑色细漂浮物(结晶β-胡萝卜素)并且在反应烧瓶的底部的壁上存在残留。
实施例3:制备饮料
将来自实施例2的0.31g乳液放入到具有50ml稳定剂和余量的水的500ml瓶中以在瓶中获得约3mg的β-胡萝卜素。所得饮料略微混浊,具有类似于黄色5号的黄色颜色并且没有可检测到的气味。
比较实施例1:用市售类胡萝卜素组合物制备饮料
将0.3g的市售类胡萝卜素组合物1CWD/Y(CAS:7235-40-7,可从巴斯夫公司商购)放入到具有余量的水的500ml瓶中以在瓶中获得约2.9mg的β-胡萝卜素。所得饮料的颜色比实施例3的饮料更显橙色,并且具有可检测到的类似胡萝卜的气味。
实施例4:制备β-胡萝卜素油悬浮液
将市售β-胡萝卜素悬浮在油中,然后装入到反应器中,并且使其在60℃到120℃的温度下保持2小时到8小时以除去小的挥发性分子。此后,在介于160℃与180℃之间的温度下对油进行热处理。将所得油制成乳液,然后进行喷雾干燥以获得粉末。
实施例5:制备β-胡萝卜素粉末
将商购β-胡萝卜素粉末在真空下在60℃到120℃的温度下保持2小时到24小时。与未经处理的粉末相比,所得粉末的感官性质得到改善。
实施例6:β-胡萝卜素组合物的气味强度的预示性分析
使用《感官评价技术》第2版Meilgaard,Civile,Carr 1991第81-88页中所述的差异测试,将1-6ppmβ-胡萝卜素的样品与对照(20-40ppm黄色5号)进行比较。样品A对应于根据实施例1制备的β-胡萝卜素组合物,而样品B、C、D和E是来自各个制造商的未经处理的市售β-胡萝卜素。每个样品和对照还含有0.1%柠檬酸、0.02%抗坏血酸和8%蔗糖。
向小组成员呈现了对照(标记为C)和随机3位数字下的样品之一,并且要求所述小组成员在0-10的范围内对与对照的差异进行排序;0为无差异,10为极端差异(N=10)。重复测试,直到每个小组成员相对于对照对每个样品进行了分析为止。结果在表4中示出。
表4
属性 | 对照 | 样品A | 样品B | 样品C | 样品D | 样品E |
平均评分 | 1.5 | 3.5 | 5.2 | 6.5 | 6.0 | 6.3 |
Claims (18)
1.一种用于改善具有挥发性杂质的类胡萝卜素组合物的感官特性的方法,所述方法包括:
将所述类胡萝卜素组合物提供到反应容器中;以及
将所述类胡萝卜素组合物保持在50℃至180℃的保持温度下,同时从所述反应容器中清除气氛,持续适于去除足够量的已挥发的引起气味的挥发性杂质的时间。
2.根据权利要求1所述的方法,其中所述清除包括将惰性气体引入到所述反应容器中,使所述反应容器经受真空或其组合。
3.根据权利要求1所述的方法,其中所述清除包括氮气喷射。
4.根据权利要求1所述的方法,其中所述清除在所述保持期间持续进行。
5.根据权利要求1所述的方法,其进一步包括使所述类胡萝卜素组合物经受130℃至250℃温度的热处理。
6.根据权利要求5所述的方法,其中所述热处理在所述保持步骤之前进行。
7.根据权利要求5所述的方法,其中所述热处理在所述保持步骤之后进行。
8.根据权利要求5所述的方法,其中所述热处理包括从所述反应容器中清除气氛。
9.根据权利要求1所述的方法,其中所述保持包括将所述类胡萝卜素组合物保持在所述保持温度下至少30分钟。
10.根据权利要求1所述的方法,其中所述保持包括将所述类胡萝卜素组合物保持在所述保持温度下1至4小时。
11.根据权利要求1所述的方法,其中所述类胡萝卜素组合物包含至少一种食用油。
12.根据权利要求1所述的方法,其中所述类胡萝卜素组合物包含至少一种抗氧化剂。
13.根据权利要求1所述的方法,其中所述类胡萝卜素组合物包含选自以下组中的至少一种类胡萝卜素:单独地或以混合物的形式,β-胡萝卜素、角黄素、虾青素、番茄红素、β-阿朴-8'-胡萝卜醛和β-阿朴-8'-胡萝卜素酸酯。
14.根据权利要求1所述的方法,其进一步包括在所述保持之后,将所述类胡萝卜素组合物调配为乳液、粉末、油性分散体或小珠的形式。
15.一种根据权利要求1所述的方法制备的类胡萝卜素食品添加剂调配物。
16.一种类胡萝卜素食品添加剂调配物,其包含气味强度值不大于5的类胡萝卜素组合物。
17.根据权利要求16所述的类胡萝卜素食品添加剂调配物,其气味强度值不大于4。
18.根据权利要求16所述的类胡萝卜素食品添加剂调配物,其中所述类胡萝卜素组合物包含至少一种合成类胡萝卜素。
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KR20050025122A (ko) * | 2001-09-13 | 2005-03-11 | 디에스엠 아이피 어셋츠 비.브이. | 식품 및 약학 조성물용 착색제 |
WO2010040683A1 (de) | 2008-10-07 | 2010-04-15 | Basf Se | Gebrauchfertige, stabile emulsion |
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- 2020-11-12 WO PCT/US2020/060099 patent/WO2021097005A1/en active Application Filing
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EP0671461A1 (en) * | 1994-03-09 | 1995-09-13 | Fuji Oil Company, Limited | Process for producing a high carotene content oil |
US5426248A (en) * | 1994-08-03 | 1995-06-20 | The Procter & Gamble Company | Stable vitamin A |
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WO2000049116A1 (en) * | 1999-02-18 | 2000-08-24 | Calgene Llc | Method for refining a seed oil having micronutrients |
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CN110178913A (zh) * | 2019-07-09 | 2019-08-30 | 广州隽沐生物科技股份有限公司 | 一种油脂组合物 |
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